Process for producing butyl and isopropyl alcohols



Patented Aug. 20, 1929.

UNITED STATES PATENT OFFICE.

Ammonia IZSAK, or cmrrmr. PARK, NEW JERSEY, ASSIGNOB TO msrnmlw ALCO- nor. conrona'rron, or wnmmeron, DELAWARE, a conrom'rron or nm-' WARE.

PROCESS FOR PRODUCING BUTYL AND ISOPBOPYL ALCOHOLS. i

No Drawing.

ring in molasses, and comprises a process of H 5 this kind in which the fermentation is brought about by a new bacterium.

An 0 ject of my invention is the successful utilization of cane molasses or beet molasses, or any fermentable hexose or pentose sugar, or other fermentable carbohydrates as a source of raw materials for the production of butyl and isopropyl alcohols. A further object of my invention is the production of. a heretofore unisolated bacterium which I have named Baoz'lfiws sacoharobutyliou/m-beta. A further object of my invention is to provide a butyl alcohol and iso- Eropyl alcohol fermentation, wherein the '7 acteria to be used may be readily isolated and kept in condition for active fermentation when inoculated into a suitable mash or medium, with excellent ield of these alcohols. A still further 0 ject of my invention is the production of acetone in the same process, but in smaller quantities than the butyl and isopropyl alcohols. jects will appear hereinafter.

The bacteria which I prefer to use, and which possess the desirable characteristics above mentioned, have been named by me Bacillus sacolzarobutylimm-beta. The manner of isolating this species of bacteria will be hereinafter described, but in order to facilitate their identification the species is described at this point in accordance with the descriptive chart of the Society of American Bacteriologists:-

Source: BarleyMalt--Meal Name: Baoil us saccharobutylz'cmn-beta.

I. Morphology.

1. Ve etative cells, motile:

filedia used-10 Brix solution of blackstrap molasses, partly neutralized Other ob- Application filed November 3, 19:27. Serial No. 231,99

2-. Sporangia:

Media used-10 Brix solution of blackstrap molasses, partly neutralized with pH-5.4. Form: Oval. Spores: Terminal. 1 Limits of size 2 to ,4 microns.

Spores will not methylene blue.

11. Oultwral features.

1. Nutrient agar slant media; age, 24 hours;

temperature 34 C. Growth: Abundant. Form of growth: Echinated. 7 Elevation of growth: Elevated.

Luster: Shiny. Optical character: Opaque. Topography: Smooth. or: Putrid. Consistency: Viscidr Media: azy. 2. Potato, 24 hours, 34 C.

" Growth: Meager.

Form of growth: In spots. Elevation of growth: Raised. T fuster: Dlpll. S o ograp y: mooth.

Colbr: White. Odor: Butyric.

111. Physical and Momma; featm'es.

' 63hours 12 hours 40 hours Gas Add calcium carbonate in excess;

stain readily with organism may be isolated:

Test tubes of ground barley malt are prepared and heated to 63 0., to saccharify the starches into maltose, and are placed in an incubator at 68 C. for 24 hours. At the end of this time, the tubes are transferred to an incubator at 35 C., and left there from 3 to a days; Bacillus saacharobutylicum-beta grows under these conditions and can be readily transferred into a fermentable hexose sugar medium for further progation. No plating is required to purify the culture, but heating to 85 C. for 15 minutes, and reincubating several times is all that is necessary.

For the production of the alcohols by means of this organism, the following examples are given for illustrative purposes:

Example I An acid mash of molasses was prepared of about 10 Brix solution of approximately 150 gallons. This acid mash o molasses may be a cane molasses which has a natural acidity, or it may be a mixture of cane and beet molasses, or it may be a beet molasses acidified- To this mash about 5 pounds of calcium carbonate was added, to neutralize or partly reduce the natural acidity of the mash, and furthermore to adjust the pH to about 5.4 to 6.8, during subsequent heating. This mash was then heated to 15 pounds pressure for about one hour, cooled off with proper care, under pure culture handling. A pressure may be maintained in the fermenter by allowing CO, or other gasses to flow into the tank either through the mash or over the mash during the cooling and setting stages. At 35 C. the mash was inoculated with Bacillus saccharobutylicum-beta, and allowed to ferment for about 72 hours, when it was found that nearly all of the sugar was exhausted or converted. The beer Was then distilled by any of the known methods.

' pressure.

approximately 150 I have found that under the best conditions a yield of total solvents of about 25 percent or more may be obtained of the sugar fermented, which is composed chiefly of butyl alcohol. The ratio of products produced by this fermentation may run as high as 75% butyl alcohol; 35% isopropyl alcohol; some acetone, and a trace of amyl and possibly of eth l alcohols.

sample Il.-An acid mash of molasses was prepared of about 10 Brix solution of gallons, rendered neutral to litmus paper in cold solution with Na CO To this mash five (5) pounds of CaCO was added, and the mash heated to 15 pounds A sample taken while hot (100 C.) indicated 7.5 pH. This mash when all wer to cool to 35 (1., showed a pH of 6.8. From this point the process was carried out similar to Example I, and gave approximately the same results.

By the term molasses mash, as used herein,

I mean to include a mixture of molasses and water. This mixture may be in the ratio of from 5 to 15 parts Water to one part molasses by volume. I have found that this ratio gives satisfactory results, but it will be understood, of course, that the ratio of dilution may exceed these figures.

The pH value of this mash may'be adjusted to the optimum point by the use of neutralizing agents, such as the carbonates or the hydroxides of the alkali or alkaline metals, ammonia, etc., for too high acidity, or say lactic acid for too low acidity.

Although the-use, of sodium carbonate or calcium carbonate is to be preferred, I may use other alkaline materials, such as barium carbonate, potassium carbonate, or strontium carbonate, sodium hydroxide, or a combination of these.

According to the process disclosed herein a special, or optimum, mash condition may f be maintained and controlled which results in an absolutely clean out normal butyl alcohol fermentation free from butyric acid contamination. Furthermore, I have found that according to this invention the special preparation of the mash to insure the desired result is simple, is positive, and can be conducted on a commercial scale without the addition or installation of expensive buildings and equipment.

By the expression maintaining and controlling the optimum conditions as used herein I mean maintaining and controlling the acidity, temperature and concentration of the medium. By foptimum temperature as used herein I mean to include temperatures of approximately 34 or 35 0.

As many apparently widely different embodiments of this invention may be made without departing from the spirit thereof, it it to be understood that I do not intend to limit myself to the specific embodiments thereof except as indicated in the appended claims.

I claim 1. A process for the manufacture of butyl and isopropyl alcohols by fermentation of a fermentable .carbohydrate medium wherein the medium is fermented by a bacillus obtained by saccharifying the starches of barley malt into maltose and incubating the maltose, said bacillus identified by its having the form of short and long rods, chain formation, rounded ends, by its dimensions of 6 to 20 microns by 2 to 3 microns, and by its property of rapid formation of spores and by its ability to produce mainly butyl and isopropyl alcohols.

2. A process for the manufacture of butyl and isopropyl alcohols by fermentation of a molasses mash medium wherein the medium is fermented by a bacillus obtained by saccharifying the starches of barley malt into maltose and incubating the maltose, said bacillus identified by its having the form of short and long rods, chain formation, rounded ends, microns by 2 to 3 microns, and b its pro erty of rapid formation of s ores and by its a ility roduce mainly utyl and isopropyl alco ols.

3. The process of roducing butyl and isopropyl alcohols and acetone, which comprises fermenting a fermentable carboydrate medium with the herein-described Bacillus saccharobutylz'mlm-beta.

4. The process of producing butyl and isoprop lalcohols and acetone which comprises ermenting a molasses mash medium with the herein-described Bacillus saccharobutylioumleta V 5. The process of producing butyl and isoprcpyl alcohols, which comprises prepa'rin a ermentable carbohydrate medium, an inoculating the medium with the herein-described Baoillus saccharobutylz'cmn-beta, and causin the medium to ferment by the action of sai; bacillus.

6. The process of producing butyl and isopropyl alcohols, which comprises preparing a mo asses mash medium, and inoculating the mash with the herein-described Bacillus saccharobutg/lic'um-beta.

7. The process of producing-butyl and isoropyl alcohols, which comprises preparing a ermentable carbohydrate medium, partially neutralizing the acidity or alkalinity of the medium, sterilizing the medium, and inoculating' the medium with the herein-described Bacillus sacckarobutg lz'cwm-beta.

8. The process of producing butyl and isopropyl alcohols which comprises fermenting a fermentable carbohydrate medium with a bacillus identified by its having the'form of short and long rods, rounded ends, chain formation, by its dimensions of 6 to 20 microns by 2 to 3 microns, by its property of rapid formation of spores and by its ability to produce mainly butyl and isopropyl alcohols in the presence of a material capable of maintaining in the sugar medium an aptimum pH value of between 5.4 and 7.

9. The process of producing but 1 and isopropyl alcohols which comprises ermenting a molasses mash medium with a bacillus identified by its having the form of short and long rods, rounded ends, chain formation, by its dimensions of 6 to 20 microns by 2 to 3 microns, by its property of rapid formation of spores and by its ability to produce mainly butyl and isopropyl alcohols in the presence of a material capable of maintaining in the sugar medium an optimum pH value of between 54 and 7.

10. In the process of producing butyl and isopropyl alcohols the steps which comprise preparing a fermentable carbohydrate medium, partially neutralizing the acidity or alkalinity of the medium, sterilizing the by its dimensions of 6 to 20' medium, cooling the medium to approximately 35 C. and inoculatin the medium with the herein-described Baczllus aaccharobutylicum-beta, allowing the fermentation to proceed to completion and distilling off said alcohols.

11. The rocess of producing butyl and isopropyl a cohols, which comprises preparing a fermentable carbohydrate medium, adding a neutralizing agent to the medium, sterilizing the medium, and inoculating the medium with the herein-described Bacillus saccharobutylz'cum-beta, and causing the medium to ferment by bacillus.

12. The process of roducing butyl and isopropyl alcohols which comprises preparing a fermentable carbohydrate medium, adding a neutralizing agent to the medium, sterilizing the medium, cooling the medium to approximately 35 C. and inoculating the medium with the herein-described Bacillus saccharobutylicmn-beta, and causing the medium to ferment by the action of said bacillus.

13. The process of producing butyl and isopropyl alcohols which comprises preparing a fermentable carbohydrate 'medium, adding a neutralizing agent to the medium, sterilizing the medium, coolin the medium to approximately 35 (1., maintaining the medium in a sterilized condition in the presthe action of said ence of an oxygeniree gas which is mert latin the medium with the herein-described B 'lus saoohaa obutg liwm-beta.

15. The rocess of producing butyl and isopropyl a cohols which'comprises preparing a fermentable carboh drate medium, adding a neutralizin material to the medium to partially neutrahze the natural acidity or alkalinity of the medium and to adjust the pH to about 5.4 to 7.0, sterilizing the medium, cooling the medium to approximately 35 0., maintaining the medium substantially free from free oxygen and inoculating the medium with the erein-described Bacillus saccharobutyliowmrbeta, and causin the mixture to ferment by the action 0% said bacillus.

16. The process of producing butyl and isopropyl alcohols which comprises. preparing a fermentable carbohydrate medium, add- 5 inoculating the medium with the herein-described Bacillus saooharobuitylimwn-beta, and causing the medium to ferment by the action of said bacillus.

17. The process of producing butyl and 10 isopropyl alcohols which comprises preparing an acid molasses medium, adding an alkaline substance taken from a group including calcium carbonate, sodium carbonate, sodium hydroxide and ammonium Hydroxide 1 to the medium, sterilizing the medium, cooling the medium to approximately 35 6, inoculating the medium with the herein-described Bacz'llus saacharobutg lz'o um-beta, and

causing the medium to ferment by the action of said bacillus. I

18. The rocess of producing butyl and isopropyl (g cohols, which com risespreparing an aci' medium of a carbo ydrate material and water, containing also an alkaline material capable of maintaining the hereindescribed optimum pH condition in the medium of 5.4 to 7.0, sterilizing the medium, inoculatin" the medium with the herein-described Hzoz'llus saocizarobu-t'yliawm bem causin the medium to ferment by the action of sai bacillus, and distilling oil the said alcohols.

In testimony whereof, I afiix my signature.

ALEXANDER IZSAK. 

